홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Diethyl Ether → Ethyl 4-(6-azaspiro(2.5)oct-6-yl)benzoate

HRID 2085717
노트
인쇄 미리보기

반응식

HRID 2085717 반응식
[CH3:1]N(N=O)C(N[N+]([O-])=O)=N.[OH-].[K+].C(OCC)C.[CH2:18]=[C:19]1[CH2:24][CH2:23][N:22]([C:25]2[CH:35]=[CH:34][C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=2)[CH2:21][CH2:20]1>C1COCC1.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH2:1]1[C:19]2([CH2:24][CH2:23][N:22]([C:25]3[CH:35]=[CH:34][C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=3)[CH2:21][CH2:20]2)[CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 16109082Ethyl 4-(4-methylenepiperidin-1-yl)benzoateHCID 135436526N-Methyl-N'-nitro-N-nitrosoguanidine

생성물 1

HCID 22729977Ethyl 4-(6-azaspiro(2.5)oct-6-yl)benzoate

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of methyl-3-nitro-1-nitrosoguanidine (1.18 g, 8.1 mmol), 40% KOH (3.4 mL), and diethyl ether (12 mL) at 0° C. was stirred for 10 minutes. The organic phase was added slowly to a −25° C. solution of Example 158C and Pd(OAc)2 (18 Mg, 0.11 mmol) in THF (8.8 mL). The mixture was stirred for 1 hour at −20° C. and concentrated. The concentrate was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate to provide the desired product. MS (DCI) m/e 260 (M+H)+.

후처리

  1. stirringThe mixture was stirred for 1 hour at −20° C.
  2. concentrationconcentrated
  3. customThe concentrate was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate

출처 및 근거

ORD 기록
ord-3210c93786f74c528de99a4d4e4d1757
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720338B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트